Search results for: Raman spectroscopy

Authors: Nadia Hammouda, K. Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, sea water

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Authors: Abdullah Faqihi, John Hedley

Abstract:

Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: laser scribing, lightscribe DVD, graphene oxide, scanning electron microscopy

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Authors: N. Boudinar, A. Djekoun, A. Otmani, B. Bouzabata, J. M. Greneche

Abstract:

High-energy ball milling is a solid-state powder processing technique that allows synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from elemental powders. The advantage of this process technology is that the powder can be produced in large quantities and the processing parameters can be easily controlled, thus it is a suitable method for commercial applications. It can also be used to produce amorphous and nanocrystalline materials in commercially relevant amounts and is also amenable to the production of a variety of alloy compositions. Mechanical alloying (high-energy ball milling) provides an inter-dispersion of elements through a repeated cold welding and fracture of free powder particles; the grain size decreases to nano metric scale and the element mix together. Progressively, the concentration gradients disappear and eventually the elements are mixed at the atomic scale. The end products depend on many parameters such as the milling conditions and the thermodynamic properties of the milled system. Here, the mechanical alloying technique has been used to prepare nano crystalline Fe_50 and Fe_64 wt.% Ni alloys from powder mixtures. Scanning electron microscopy (SEM) with energy-dispersive, X-ray analyses and Mössbauer spectroscopy were used to study the mixing at nanometric scale. The Mössbauer Spectroscopy confirmed the ferromagnetic ordering and was use to calculate the distribution of hyperfin field. The Mössbauer spectrum for both alloys shows the existence of a ferromagnetic phase attributed to γ-Fe-Ni solid solution.

Keywords: nanocrystalline, mechanical alloying, X-ray diffraction, Mössbauer spectroscopy, phase transformations

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Authors: S. V. Prabhakar Vattikuti, Chan Byon

Abstract:

In this paper, we report a facile synthetic strategy of randomly disturbed Bi₂S₃ nanorods on WS₂ nanosheets, which are synthesized via a controlled hydrothermal method without surfactant under an inert atmosphere. We developed a simple hydrothermal method for the formation of heterostructured of Bi₂S₃/WS₂ with a large scale (>95%). The structural features, composition, and morphology were characterized by XRD, SEM-EDX, TEM, HRTEM, XPS, UV-vis spectroscopy, N₂ adsorption-desorption, and TG-DTA measurements. The heterostructured Bi₂S₃/WS₂ composite has significant photocatalytic efficiency toward the photodegradation of organic dye. The time-dependent UV-vis absorbance spectroscopy measurement was consistent with the enhanced photocatalytic degradation of rhodamine B (RhB) under visible light irradiation with the diminishing carrier recombination for the Bi₂S₃/WS₂ photocatalyst. Due to their marked synergistic effects, the supported Bi₂S₃ nanorods on WS₂ nanosheet heterostructures exhibit significant visible-light photocatalytic activity and stability for the degradation of RhB. A possible reaction mechanism is proposed for the Bi₂S₃/WS₂ composite.

Keywords: photocatalyst, heterostructures, transition metal disulfides, organic dye, nanorods

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Authors: N. Hammouda, K. Belmokre

Abstract:

The paints are used extensively today in the industry to protect the metallic structures of the aggressive environments. This work is devoted to the study of corrosion resistance and aging behavior of a paint coating providing external protection for oil tankers. To avoid problems related to corrosion of these vessels, two protection modes are provided: An electro chemical active protection (cathodic protection of the hull). A passive protection by external painting. Investigations are conducted using stationary and non-stationary electro chemical tools such as electro chemical impedance spectroscopy has allowed us to characterize the protective qualities of these films. The application of the EIS on our damaged in-situ painting shows the existence of several capacitive loops which is an indicator of the failure of our tested paint. Microscopic analysis (micrograph) helped bring essential elements in understanding the degradation of our paint condition and immersion training corrosion products.

Keywords: epoxy paints, electrochemical impedance spectroscopy, corrosion mechanisms, seawater

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Authors: Nadia Hammouda, Kamel Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, sea water

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Authors: Theo H. G. Moundzounga

Abstract:

Arsenic and 2-chlorophenol are priority pollutants that pose serious health threats to humans and ecology. An electrochemical sensor, based on graphitic carbon nitride (g-C₃N₄) and carbon dots (CDs), was fabricated and used for the determination of arsenic and 2-chlorophenol. The g-C₃N₄/CDs nanocomposite was prepared via microwave irradiation heating method and was dropped-dried on the surface of the glassy carbon electrode (GCE). Transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence (PL), Fourier transform infrared spectroscopy (FTIR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) were used for the characterization of structure and morphology of the nanocomposite. Electrochemical characterization was done by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical behaviors of arsenic and 2-chlorophenol on different electrodes (GCE, CDs/GCE, and g-C₃N₄/CDs/GCE) was investigated by differential pulse voltammetry (DPV). The results demonstrated that the g-C₃N₄/CDs/GCE significantly enhanced the oxidation peak current of both analytes. The analytes detection sensitivity was greatly improved, suggesting that this new modified electrode has great potential in the determination of trace level of arsenic and 2-chlorophenol. Experimental conditions which affect the electrochemical response of arsenic and 2-chlorophenol were studied, the oxidation peak currents displayed a good linear relationship to concentration for 2-chlorophenol (R²=0.948, n=5) and arsenic (R²=0.9524, n=5), with a linear range from 0.5 to 2.5μM for 2-CP and arsenic and a detection limit of 2.15μM and 0.39μM respectively. The modified electrode was used to determine arsenic and 2-chlorophenol in spiked tap and effluent water samples by the standard addition method, and the results were satisfying. According to the measurement, the new modified electrode is a good alternative as chemical sensor for determination of other phenols.

Keywords: electrochemistry, electrode, limit of detection, sensor

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Authors: Mai M. Khalaf, Hany M. Abd El-Lateef

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A new good application for the sol gel method is to improve the corrosion inhibition properties of carbon steel by the dip coating method of Nano TiO2 films and its modification with Poly Ethylene Glycol (PEG). The prepared coating samples were investigated by different techniques, X-ray diffraction, Scanning Electron Microscopy (SEM), transmission electron microscopy and Energy Dispersive X-ray Spectroscopy (EDAX). The corrosion inhibition performance of the blank carbon steel and prepared coatings samples were evaluated in 0.5 M H2SO4 by using Electrochemical Impedance Spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that corrosion resistance of carbon steel increases with increasing the number of coated layers of both nano–TiO2 films and its modification of PEG. SEM-EDAX analyses confirmed that the percentage atomic content of iron for the carbon steel in 0.5 M H2SO4 is 83% and after the deposition of the steel in nano TiO2 sol and that with PEG are 94.3% and 93.7% respectively.

Keywords: dip-coatings, corrosion protection, sol gel, TiO2 films, PEG

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Authors: Andile Mkhohlakali, Tien-Chien Jen, James Tshilongo, Happy Mabowa

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Among different parameters, oxygen is one of the most important analytes of interest, dissolved oxygen (DO) concentration is very crucial and significant for various areas of physical, chemical, and environmental monitoring. Herein we report oxygen-sensitive luminophores -based lanthanum(III) trifluoromethanesulfonate), [La]³⁺ was encapsulated into SiO₂-based xerogel matrix. The nanosensor is composed of organically modified silica nanoparticles, doped with the luminescent oxygen–sensitive lanthanum(III) trifluoromethanesulfonate complex. The precursor materials used for sensing film were triethyl ethoxy silane (TEOS) and (3-Mercaptopropyltriethoxysilane) (MPTMS- TEOS) used for SiO2-baed matrices. Brunauer–Emmett–Teller (BET), and BJH indicate that the SiO₂ transformed from microporous to mesoporous upon the addition of La³⁺ luminophore with increased surface area (SBET). The typical amorphous SiO₂ based xerogels were revealed with X-Ray diffraction (XRD) and Selected Area Electron Diffraction (SAED) analysis. Scanning electron microscope- (SEM) and transmission electron microscope (TEM) showed the porous morphology and reduced particle for SiO₂ and La-SiO₂ xerogels respectively. The existence of elements, siloxane networks, and thermal stability of xerogel was confirmed by energy dispersive spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), and Thermographic analysis (TGA). UV-Vis spectroscopy and photoluminescence (PL) have been used to characterize the optical properties of xerogels. La-SiO₂ demonstrates promising characteristic features of an active sensing film for dissolved oxygen in the water. Keywords: Sol-gel, ORMOSILs, encapsulation, Luminophores quenching, O₂-sensing

Keywords: sol-gel, ORMOSILs, luminophores quenching, O₂-sensing

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Authors: Jyoti Yadav, Rini Singh, Anoop M.D, Nisha Yadav, N. Srinivasa Rao, Fouran Singh, Takayuki Ichikawa, Ankur Jain, Kamlendra Awasthi, Manoj Kumar

Abstract:

Nanocrystalline films exhibit defects and strain induced by its grain boundaries. Defects and strain affect the physical as well as topological insulating properties of the Bi2Te3 thin films by changing their electronic structure. In the present studies, the effect of Ni7+ ion irradiation on the physical and electrical properties of Bi2Te3 thin films was studied. The films were irradiated at five different fluences (5x1011, 1x1012, 3x1012, 5x1012, 1x1013 ions/cm2). Thin films synthesized using the e-beam technique possess a rhombohedral crystal structure with the R-3m space group. The average crystallite size, as determined by x-ray diffraction (XRD) peak broadening, was found to be 18.5 ± 5 (nm). It was also observed that irradiation increases the induced strain. Raman Spectra of the films demonstrate the splitting of A_1u^1 modes originating from the vibrations along the c-axis. This is by the variation in the lattice parameter ‘c,’ as observed through XRD. The atomic force microscopy study indicates the decrease in surface roughness up to the fluence of 3x1012 ions/cm2 and further increasing the fluence increases the roughness. The decrease in roughness may be due to the growth of smaller nano-crystallites on the surface of thin films due to irradiation-induced annealing. X-ray photoelectron spectroscopy studies reveal the composition to be in close agreement to the nominal values i.e. Bi2Te3. The resistivity v/s temperature measurements revealed an increase in resistivity up to the fluence 3x1012 ions/cm2 and a decrease on further increasing the fluence. The variation in electrical resistivity is corroborated with the change in the carrier concentration as studied through low-temperature Hall measurements. A crossover from the n-type to p-type carriers was achieved in the irradiated films. Interestingly, tuning of the Fermi level by compensating the bulk carriers using ion-irradiation could be achieved.

Keywords: Annealing, Irradiation, Fermi level, Tuning

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Authors: Omar Concepcion, Osvaldo De Melo, Arturo Escobosa

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Topological insulator (TI) materials are insulating in the bulk and conducting in the surface. The unique electronic properties associated with these surface states make them strong candidates for exploring innovative quantum phenomena and as practical applications for quantum computing, spintronic and nanodevices. Many materials, including Bi₂Te₃, have been proposed as TIs and, in some cases, it has been demonstrated experimentally by angle-resolved photoemission spectroscopy (ARPES), scanning tunneling spectroscopy (STM) and/or magnetotransport measurements. A clean surface is necessary in order to make any of this measurements. Several techniques have been used to produce films and different kinds of nanostructures. Growth and characterization in situ is usually the best option although cleaving the films can be an alternative to have a suitable surface. In the present work, we report a comparison of Bi₂Te₃ grown by physical vapor transport (PVT) and molecular beam epitaxy (MBE). The samples were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and ARPES. The Bi₂Te₃ samples grown by PVT, were cleaved in the ultra-high vacuum in order to obtain a surface free of contaminants. In both cases, the XRD shows a c-axis orientation and the pole diagrams proved the epitaxial relationship between film and substrate. The ARPES image shows the linear dispersion characteristic of the surface states of the TI materials. The samples grown by PVT, a relatively simple and cost-effective technique shows the same high quality and TI properties than the grown by MBE.

Keywords: Bismuth telluride, molecular beam epitaxy, physical vapor transport, topological insulator

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Authors: Bhargav Baruah, Ali Shemsedin Reshad, Pankaj Tiwari

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This work presents a detailed study on the thermal degradation kinetics of co-pyrolysis of oil shale of Upper Assam, India with rubber seed shell, and lab-scale pyrolysis to investigate the influence of pyrolysis parameters on product yield and composition of products. The physicochemical characteristics of oil shale and rubber seed shell were studied by proximate analysis, elemental analysis, Fourier transform infrared spectroscopy and X-ray diffraction. The physicochemical study showed the mixture to be of low moisture, high ash, siliceous, sour with the presence of aliphatic, aromatic, and phenolic compounds. The thermal decomposition of the oil shale with rubber seed shell was studied using thermogravimetric analysis at heating rates of 5, 10, 20, 30, and 50 °C/min. The kinetic study of the oil shale pyrolysis process was performed on the thermogravimetric (TGA) data using three model-free isoconversional methods viz. Friedman, Flynn Wall Ozawa (FWO), and Kissinger Akahira Sunnose (KAS). The reaction mechanisms were determined using the Criado master plot. The understanding of the composition of Indian oil shale and rubber seed shell and pyrolysis process kinetics can help to establish the experimental parameters for the extraction of valuable products from the mixture. Response surface methodology (RSM) was employed usinf central composite design (CCD) model to setup the lab-scale experiment using TGA data, and optimization of process parameters viz. heating rate, temperature, and particle size. The samples were pre-dried at 115°C for 24 hours prior to pyrolysis. The pyrolysis temperatures were set from 450 to 650 °C, at heating rates of 2 to 20°C/min. The retention time was set between 2 to 8 hours. The optimum oil yield was observed at 5°C/min and 550°C with a retention time of 5 hours. The pyrolytic oil and gas obtained at optimum conditions were subjected to characterization using Fourier transform infrared spectroscopy (FT-IR) gas chromatography and mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR).

Keywords: Indian oil shale, rubber seed shell, co-pyrolysis, isoconversional methods, gas chromatography, nuclear magnetic resonance, Fourier transform infrared spectroscopy

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Authors: Kohei Yamamoto, Jae-Ho Kim, Susumu Yonezawa

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The surface of polyethylene terephthalate (PET) was modified with fluorine gas at 25 ℃ and 100 Torr for one h. Moreover, the effect of ethanol washing on surface modification was investigated in this study. The surface roughness of the fluorinated and washed PET samples was approximately six times larger than that (0.6 nm) of the untreated thing. The results of Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy showed that the bonds such as -C=O and -C-Hx derived from raw PET decreased and were converted into fluorinated bonds such as -CFx after surface fluorination. Even after washing with ethanol, the fluorinated bonds stably existed on the surface. These fluorinated bonds showed higher electronegativity according to the zeta potential results. The negative surface charges were increased by washing the ethanol, and it caused to increase in the number of polar groups such as -CHF- and -C-Fx. The fluorinated and washed surface of PET could promote the adsorption of Ag+ ions in AgNO₃ solution because of the increased surface roughness and the negatively charged surface.

Keywords: Ag+ ions adsorption, polyethylene terephthalate, surface fluorination, zeta potential

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Authors: Surabhi Pandey, Pavuluri Srinivasa Rao

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Extrusion processing is a high-temperature short time (HTST) treatment which can improve protein quality and digestibility together with retaining active nutrients. In-vitro protein digestibility of plant protein-based foods is generally enhanced by extrusion. The current study aimed to investigate the effect of extrusion cooking on in-vitro protein digestibility (IVPD) and conformational modification of protein in green banana flour extrudates. Green banana flour was extruded through a co-rotating twin-screw extruder varying the moisture content, barrel temperature, screw speed in the range of 10-20 %, 60-80 °C, 200-300 rpm, respectively, at constant feed rate. Response surface methodology was used to optimise the result for IVPD. Fourier-transform infrared spectroscopy (FTIR) analysis provided a convenient and powerful means to monitor interactions and changes in functional and conformational properties of extrudates. Results showed that protein digestibility was highest in extrudate produced at 80°C, 250 rpm and 15% feed moisture. FTIR analysis was done for the optimised sample having highest IVPD. FTIR analysis showed that there were no changes in primary structure of protein while the secondary protein structure changed. In order to explain this behaviour, infrared spectroscopy analysis was carried out, mainly in the amide I and II regions. Moreover, curve fitting analysis showed the conformational changes produced in the flour due to protein denaturation. The quantitative analysis of the changes in the amide I and II regions provided information about the modifications produced in banana flour extrudates.

Keywords: extrusion, FTIR, protein conformation, raw banana flour, SDS-PAGE method

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Authors: M. S. Gaafar, S. Y. Marzouk

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Sodium borosilicate glasses doped with different content of NdF3 mol % have been prepared by rapid quenching method. Ultrasonic velocities (both longitudinal and shear) measurements have been carried out at room temperature and at ultrasonic frequency of 4 MHz. Elastic moduli, Debye temperature, softening temperature and Poisson's ratio have been obtained as a function of NdF3 modifier content. Results showed that the elastic moduli, Debye temperature, softening temperature and Poisson's ratio have very slight change with the change of NdF3 mol % content. Based on FTIR spectroscopy and theoretical (Bond compression) model, quantitative analysis has been carried out in order to obtain more information about the structure of these glasses. The study indicated that the structure of these glasses is mainly composed of SiO4 units with four bridging oxygens (Q4), and with three bridging and one nonbridging oxygens (Q3).

Keywords: borosilicate glasses, ultrasonic velocity, elastic moduli, FTIR spectroscopy, bond compression model

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Authors: Stephen Daniel Iduh, Evans Chidi Egwin, Oluwatosin Kudirat Shittu

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The process for the development of reliable and eco-friendly metallic Nanoparticles is an important step in the field of Nanotechnology for biomedical application. To achieve this, use of natural sources like biological systems becomes essential. In the present work, extracellular biosynthesis of gold Nanoparticles using aqueous leave and stembark extracts of K. senegalensis has been attempted. The gold Nanoparticles produced were characterized using High Resolution scanning electron microscopy, Ultra Violet–Visible spectroscopy, zeta-sizer Nano, Energy-Dispersive X-ray (EDAX) Spectroscopy and Fourier Transmission Infrared (FTIR) Spectroscopy. The cytotoxicity of the synthesized gold nanoparticles on MCF-7 cell line was evaluated using MTT assay. The result showed a rapid development of Nano size and shaped particles within 5 minutes of reaction with Surface Plasmon Resonance at 520 and 525nm respectively. An average particle size of 20-90nm was confirmed. The amount of the extracts determines the core size of the AuNPs. The core size of the AuNPs decreases as the amount of extract increases and it causes the shift of Surface Plasmon Resonance band. The FTIR confirms the presence of biomolecules serving as reducing and capping agents on the synthesised gold nanoparticles. The MTT assay shows a significant effect of gold nanoparticles which is concentration dependent. This environment-friendly method of biological gold Nanoparticle synthesis has the potential and can be directly applied in cancer therapy.

Keywords: biosynthesis, gold nanoparticles, characterization, calotropis procera, cytotoxicity

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Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky

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The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

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Authors: Setareh Shekarsaraei, Marjan Moridi, Nasser L. Hadipour

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In this study, nuclear magnetic resonance spectroscopy and nuclear quadrupole resonance spectroscopy parameters of 14N (Nitrogen in imidazole ring) in N–H…O hydrogen bonding for Histidine hydrochloride monohydrate were calculated via density functional theory. We considered a five-molecule model system of Histidine hydrochloride monohydrate. Also, we examined the trends of environmental effect on hydrogen bonds as well as cooperativity. The functional used in this research is M06-2X which is a good functional and the obtained results have shown good agreement with experimental data. This functional was applied to calculate the NMR and NQR parameters. Some correlations among NBO parameters, NMR, and NQR parameters have been studied which have shown the existence of strong correlations among them. Furthermore, the geometry optimization has been performed using M062X/6-31++G(d,p) method. In addition, in order to study cooperativity and changes in structural parameters, along with increase in cluster size, natural bond orbitals have been employed.

Keywords: hydrogen bonding, density functional theory (DFT), natural bond orbitals (NBO), cooperativity effect

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Authors: Ljerka Kratofil Krehula, Vanja Gilja, Andrea Husak, Sniježana Šuka, Zlata Hrnjak-Murgić

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Zinc oxide (ZnO) can be used as photocatalysts for water purification. However, one particular interest is given on the integration of inorganic ZnO nanoclusters with conducting polymers because the resulting nanocomposites may possess unique properties and enhanced photocatalytic activity in comparison to pure ZnO, using UV and also visible light. It is needed to explore the appropriate structure of polypyrrole that can induce activation of ZnO photocatalyst since the synthesis of organic/inorganic hybrid materials can result in a synergistic and complementary feature, increasing ZnO photocatalytic efficiency. In this paper several different composites of polypyrrole/zinc oxide (ZnO) were studied. Composite samples were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and scanning electron microscopy (SEM). The photocatalytic efficiency of prepared samples was studied as a decomposition of Reactive Red 45 (RR 45) dye, which was monitored by UV-Vis spectroscopy as a change in absorbance of characteristic wavelength at 542 nm. Results show good photocatalytic efficiency of all nanocomposite samples.

Keywords: photocatalysis, polypyrrole, wastewater, zinc oxide

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Authors: Prasanta Sutradhar, Mitali Saha

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With an increasing awareness of green and clean energy, zinc oxide based solar cells were found to be suitable candidates for cost-effective and environmentally friendly energy conversion devices. In this work, we have reported the green synthesis of zinc oxide nanoparticles (ZnO) by thermal method and under microwave irradiation using the aqueous extract of tomatoes as non-toxic and ecofriendly reducing material. The synthesized ZnO nanoparticles were characterised by UV-Visible spectroscopy (UV-Vis), infra-red spectroscopy (IR), particle size analyser (DLS), scanning electron microscopy (SEM), atomic force microscopy (AFM), and X- ray diffraction study (XRD). A series of ZnO nanocomposites with titanium dioxide nanoparticles (TiO2) and graphene oxide (GO) were prepared for photovoltaic application. Structural and morphological studies of these nanocomposites were carried out using UV-vis, SEM, XRD, and AFM. The current-voltage measurements of the nanocomposites demonstrated enhanced power conversion efficiency of 6.18% in case of ZnO/GO/TiO2 nanocomposite.

Keywords: ZnO, green synthesis, microwave, nanocomposites, I-V characteristics

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Authors: Ayu Minamizawa, Jae-Ho Kim, Susumu Yonezawa

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Aqueous peroxotitanium acid solution was prepared by the reaction between H₂O₂ solution and TiO₂ fluorinated using F₂ gas. The coating of TiO₂/SiO₂ multilayer on the surface of polycarbonate (PC) resin was carried out step by step using the TEOS solution and aqueous peroxotitanium acid solution. We confirmed each formation of SiO₂ and TiO₂ layer by scanning electron microscopy and energy-dispersive X-ray spectroscopy, and x-ray photoelectron spectroscopy results. The formation of a TiO₂ thin layer on SiO₂ coated on polycarbonate (PC) was carried out at 120 ℃ and for 15 min ~ 3 h with aqueous peroxotitanium acid solution using a hydrothermal synthesis autoclave reactor. The morphology TiO₂ coating layer largely depended on the reaction time, as shown in the results of SEM-EDS analysis. Increasing the reaction times, the TiO₂ layer expanded uniformly. Moreover, the surface fluorination of the SiO₂ layer can promote the formation of the TiO₂ layer on the surface.

Keywords: aqueous peroxotitanium acid solution, photocatalytic activity, polycarbonate, surface fluorination

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Authors: Łukasz Mazur, Kamil Domaradzki, Maciej Bik, Tomasz Brylewski, Aleksander Gil

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Interconnects used in solid oxide fuel and electrolyzer cells (SOFCₛ/SOECs) serve several important functions, and therefore interconnect materials must exhibit certain properties. Their thermal expansion coefficient needs to match that of the ceramic components of these devices – the electrolyte, anode and cathode. Interconnects also provide structural rigidity to the entire device, which is why interconnect materials must exhibit sufficient mechanical strength at high temperatures. Gas-tightness is also a prerequisite since they separate gas reagents, and they also must provide very good electrical contact between neighboring cells over the entire operating time. High-chromium ferritic steels meets these requirements to a high degree but are affected by the formation of a Cr₂O₃ scale, which leads to increased electrical resistance. The final criterion for interconnect materials is chemical inertness in relation to the remaining cell components. In the case of ferritic steels, this has proved difficult due to the formation of volatile and reactive oxyhydroxides observed when Cr₂O3 is exposed to oxygen and water vapor. This process is particularly harmful on the cathode side in SOFCs and the anode side in SOECs. To mitigate this, protective-conducting ceramic coatings can be deposited on an interconnect's surface. The area-specific resistance (ASR) of a single interconnect cannot exceed 0.1 m-2 at any point of the device's operation. The rate at which the CrO₃ scale grows on ferritic steels can be reduced significantly via the so-called reactive element effect (REE). Research has shown that the deposition of Gd₂O₃ nanoparticles on the surface of the Crofer 22 APU, already modified using a protective-conducting spinel layer, further improves the oxidation resistance of this steel. However, the deposition of the manganese-cobalt spinel layer is a rather complex process and is performed at high temperatures in reducing and oxidizing atmospheres. There was thus reason to believe that this process may reduce the effectiveness of Gd₂O₃ nanoparticles added as an active element source. The objective of the present study was, therefore, to determine any potential impact by introducing a preoxidation stage after the nanoparticle deposition and before the steel is coated with the spinel. This should have allowed the nanoparticles to incorporate into the interior of the scale formed on the steel. Different samples were oxidized for 7000 h in air at 1073 K under quasi-isothermal conditions. The phase composition, chemical composition, and microstructure of the oxidation products formed on the samples were determined using X-ray diffraction, Raman spectroscopy, and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy. A four-point, two-probe DC method was applied to measure ASR. It was found that coating deposition does indeed reduce the beneficial effect of Gd₂O₃ addition, since the smallest mass gain and the lowest ASR value were determined for the sample for which the additional preoxidation stage had been performed. It can be assumed that during this stage, gadolinium incorporates into and segregates at grain boundaries in the thin Cr₂O₃ that is forming. This allows the Gd₂O₃ nanoparticles to be a more effective source of the active element.

Keywords: interconnects, oxide nanoparticles, reactive element effect, SOEC, SOFC

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Authors: Kwame Sarkodie, William Cheung, Andrew R. Fergursson

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The characterization of multiphase flow has gained enormous attention for most petroleum and chemical industrial processes. In order to fully characterize fluid phases in a stream or containment, there needs to be a profound knowledge of the existing composition of fluids present. This introduces a problem for real-time monitoring of fluid dynamics such as fluid distributions, and phase fractions. This work presents a simple technique of correlating absorbance spectrums of water, oil and air bubble present in containment. These spectra absorption outputs are derived by using an Fourier Infrared spectrometer. During the testing, air bubbles were introduced into static water column and oil containment and with light absorbed in the infrared regions of specific wavelength ranges. Attenuation coefficients are derived for various combinations of water, gas and oil which reveal the presence of each phase in the samples. The results from this work are preliminary and viewed as a build up to the design of a multiphase flow rig which has an infrared sensor pair to be used for multiphase flow characterization.

Keywords: attenuation, infrared, multiphase, spectroscopy

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Authors: Jibon Sharma, Alakjyoti Patowary, Moirangthem Nara Singh

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In experimental research it is very much essential to obtain the quality control of the system used for the experiment. NaI (Tl) scintillation detector is the most commonly used in radiation and medical physics for measurement of the gamma ray activity of various samples. In addition, the scintillation detector has a lot of applications in the elemental analysis of various compounds, alloys using activation analysis. In each application for quantitative analysis, it is very much essential to know the detection efficiency and resolution for different gamma energies. In this work, the energy dependence of efficiency and resolution of NaI (Tl) detector using gamma-ray spectroscopy are investigated. Different photon energies of 356.01 keV,511keV,661.60keV,1170 keV,1274.53 keV and 1330 keV are obtained from four radioactive sources (133Ba,22Na,137Cs and 60 Co) used in these studies. Values of full energy peak efficiencies of these gamma energies are found to be respectively 58.46%,10.15%,14.39%,1.4%,3.27% and 1.31%. The values of percent resolution for above different gamma ray energies are found to be 11.27%,7.27%,6.38%,5.17%,4.86% and 4.74% respectively. It was found that the efficiency of the detector exponentially decreases with energy and the resolution of the detector is directly proportional to the energy of gamma-ray.

Keywords: naI (Tl) gamma-ray spectrometer, resolution, full energy peak efficiency, radioactive sources

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Authors: Ouafek Nora, Keghouche Nassira, Dehdouh Heider, Untidt Carlos

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A lot of knowledge has been accumulated on the metal clusters supported on oxide surfaces because of their multiple applications in microelectronics, heterogeneous catalysis, and magnetic devices. In this work, the surface state of Ni / MgO has been studied by XPS (X-ray Photoemission Spectroscopy). The samples were prepared by impregnation with ion exchange Ni²⁺ / MgO, followed by either a thermal treatment in air (T = 100 -350 ° C) or a gamma irradiation (dose 100 kGy, 25 kGy dose rate h -1). The obtained samples are named after impregnation NMI, NMR after irradiation, and finally NMC(T) after calcination at the temperature T (T = 100-600 °C). A structural study by XRD and HRTEM reveals the presence of nanoscaled Ni-Mg intermetallic phases (Mg₂Ni, MgNi₂, and Mg₆Ni) and magnesium hydroxide. Mg(OH)₂ in nanometric range (2- 4 nm). Mg-Ni compounds are of great interest in energy fields (hydrogen storage…). XPS spectra show two Ni2p peaks at energies of about 856.1 and 861.9 eV, indicating that the nickel is primarily in an oxidized state on the surface. The shift of the main peak relative to the pure NiO (856.1 instead of 854.0 eV) suggests that in addition to oxygen, nickel is engaged in another link with magnesium. This is in agreement with the O1s spectra which present an overlap of peaks corresponds to NiO and MgO, at a calcination temperature T ≤ 300 °C.

Keywords: XPS, XRD, nanoparticules, Ni-MgO

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Pachari Chuenta, Suwat Nanan

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ZnO nanostructures have been synthesized successfully in high yield via catalyst-free chemical precipitation technique by varying zinc source (either zinc nitrate or zinc acetate) and oxygen source (either oxalic acid or urea) without using any surfactant, organic solvent or capping agent. The ZnO nanostructures were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), UV-vis diffuse reflection spectroscopy (UV-vis DRS), and photoluminescence spectroscopy (PL). The FTIR peak in the range of 450-470 cm-1 corresponded to Zn-O stretching in ZnO structure. The synthesized ZnO samples showed well crystalized hexagonal wurtzite structure. SEM micrographs displayed spherical droplet of about 50-100 nm. The band gap of prepared ZnO was found to be 3.4-3.5 eV. The presence of PL peak at 468 nm was attributed to surface defect state. The photocatalytic activity of ZnO was studied by monitoring the photodegradation of reactive red (RR141) azo dye under ultraviolet (UV) light irradiation. Blank experiment was also separately carried out by irradiating the aqueous solution of the dye in absence of the photocatalyst. The initial concentration of the dye was fixed at 10 mgL-1. About 50 mg of ZnO photocatalyst was dispersed in 200 mL dye solution. The sample was collected at a regular time interval during the irradiation and then was analyzed after centrifugation. The concentration of the dye was determined by monitoring the absorbance at its maximum wavelength (λₘₐₓ) of 544 nm using UV-vis spectroscopic analysis technique. The sources of Zn and O played an important role on photocatalytic performance of the ZnO photocatalyst. ZnO nanoparticles which prepared by zinc acetate and oxalic acid at molar ratio of 1:1 showed high photocatalytic performance of about 97% toward photodegradation of reactive red azo dye (RR141) under UV light irradiation for only 60 min. This work demonstrates the promising potential of ZnO nanomaterials as photocatalysts for environmental remediation.

Keywords: azo dye, chemical precipitation, photocatalytic, ZnO

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Authors: Ajay Krishnamurthy, Mariyappan Mahesh Kumar, Sellamuthu Periyar Selvam

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Fruits are considered as functional foods due to the presence of various bioactive compounds available such as polyphenols, which are beneficial to health when consumed as part of our diet. The primary objective of this study was to analyze the various functional groups present in ethanolic extracts of Hylocereus undatus and Garcinia indica and also measure their antibacterial and antioxidant potential respectively thereby affirming its nutraceutical potential. To fulfill our objective, a Fourier - transform Infrared Spectroscopy (FTIR) was conducted for functional group analysis, Total Phenolic Content and DPPH free radical scavenging activity for measuring it anti-oxidant potential and agar-well diffusion assay for antibacterial potential. On careful observation and analysis of the spectrum it was found that both the fruit extracts contain similar compounds viz. Phenols, Alkanes, Alkenes, Aldehydes, Ketones, Carboxylic Acid and Amines. Total phenolic content of H.undatus and G.indica was estimated to be (26.85 ± 1.84 mg GAE/100g) and (32.84 ± 1.63 mg GAE/100g) respectively which corresponds to an inhibition of 84% and 81% respectively. H.undatus shows an inhibition of (3.4 ± 2.1mm) in gram-positive and (4.2 ± 2.24mm) in gram-negative organism on the other hand G.indica shows (2.1 ± 0.98mm) in gram-positive and (3.1 ± 1.44mm) in gram negative. The presence of such diverse compounds in the fruits helps us to understand the necessity for the inclusion of fruits in our daily diet and also helps the pharmaceutical industry in realizing the importance of exotic fruits as a potential nutraceutical.

Keywords: DPPH, fourier-transform infrared spectroscopy (FTIR), Hylocereus undatus, Garcinia indica

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Authors: R. Sharma, A. Sil, S. Ray

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Nanocomposites gel polymer electrolytes are gaining more and more attention among the researchers worldwide due to their possible applications in various electrochemical devices particularly in solid-state Li-ion batteries. In this work we have investigated the effect of nanofibers on the electrical properties of PVDF-HFP based gel electrolytes. The nanocomposites polymer electrolytes have been synthesized by solution casting technique with 10wt% of ZrO2. By analysis of impedance spectroscopy it has been demonstrated that the incorporation of ZrO2 into PVDF-HFP–(PC+DEC)–LiClO4 gel polymer electrolyte system significantly enhances the ionic conductivity of the electrolyte. The enhancement of ionic conductivity seems to be correlated with the fact that the dispersion of ZrO2 to PVDF-HFP prevents polymer chain reorganization due to the high aspect ratio of ZrO2, resulting in reduction in polymer crystallinity, which gives rise to an increase in ionic conductivity. The decrease of crystallinity of PVDF-HFP due the addition of ZrO2 has been confirmed by XRD. The interaction of ZrO2 with various constituents of polymer electrolytes has been studied by FTIR spectroscopy. TEM results show that the fillers (ZrO2) has distributed uniformly in the polymer electrolytes. Moreover, ZrO2 added gel polymer electrolytes offer better thermal stability as compared to that of ZrO2 free electrolytes as confirmed by TGA analysis.

Keywords: polymer electrolytes, ZrO2, ionic conductivity, FTIR

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Authors: Mauricio A. Sarabia-Vallejos, Carmen M. Gonzalez-Henriquez, Adolfo Del Campo-Garcia, Aitzibier L. Cortajarena, Juan Rodriguez-Hernandez

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In this study, it was explored the formation and the morphological differences between wrinkled hydrogel patterns obtained via generation of surface instabilities. The slight variations in the polymerization conditions produce important changes in the material composition and pattern structuration. The compounds were synthesized using three main components, i.e. an amphiphilic monomer, hydroxyethyl methacrylate (HEMA), a hydrophobic monomer, trifluoroethyl methacrylate (TFMA), and a hydrophilic crosslinking agent, poly(ethylene glycol) diacrylate (PEGDA). The first part of this study was related to the formation of wrinkled surfaces using only HEMA and PEGDA and varying the amount of water added in the reaction. The second part of this study involves the gradual insertion of TFMA into the hydrophilic reaction mixture. Interestingly, the manipulation of the chemical composition of this hydrogel affects both surface morphology and physicochemical characteristics of the patterns, inducing transitions from one particular type of structure (wrinkles or ripples) to different ones (creases, folds, and crumples). Contact angle measurements show that the insertion of TFMA produces a slight decrease in surface wettability of the samples, remaining however highly hydrophilic (contact angle below 45°). More interestingly, by using confocal Raman spectroscopy, important information about the wrinkle formation mechanism is obtained. The procedure involving two consecutive thermal and photopolymerization steps lead to a “pseudo” two-layer system. Thus, upon photopolymerization, the surface is crosslinked to a higher extent than the bulk and water evaporation drives the formation of wrinkled surfaces. Finally, cellular, and bacterial proliferation studies were performed to the samples, showing that the amount of TFMA included in each sample slightly affects the proliferation of both (bacteria and cells), but in the case of bacteria, the morphology of the sample also plays an important role, importantly reducing the bacterial proliferation.

Keywords: antibiofouling properties, hydrophobic/hydrophilic balance, morphologic characterization, wrinkled hydrogel patterns

Procedia PDF Downloads 163